Process of forming colloid products



p 20, 1927. s. A NEIDICH 64 80 PROCESS OF FORMING COLLOID PRODUCTS Filed March :5. 1926 FIGI l/V Vf/V 70R: Janus; A. Nun/en,

Patented Sept. 20, 1927.

UNITED STATES PATENT OFFICE.

SAMUEL A. NEIDIGH, OF EDGEWATEB PARK, NEW JERSEY.

PROCESS OI FORMING COLLOID PRODUCTS.

Application filed March 3, 1926. Serial No. 91,962.

My invention is applicable in the manufacture of filaments by pro'ectin viscose (cellulose sulphocarbonate) t rougli orifices into baths containing chemicals which coagulate the viscose as a semi-solid impure cellulose hydrate of sufiicient strength to be manipulated in the subsequent operations of dyeing, drying, and weaving or braiding the same. Ordinaril filaments projected through circular ori ces and thus treated are solid cylinders of substantially uniform diameter and smooth exterior when dried. However, the pur ose and effect of this invention is to pro uce a solid substantially uniform cylin rical filament surrounded by a tubular sheath which is crinkled so that its exterior surface resents numerous facets for reflection of lig t so as to have a scintillating effect, which is particularly desirable in the formations of braids, cords, etc., used in the millinery trade.

As hereinafter described; my invention includes the extrusion of rimarily solid filaments of viscose, througl l suitable spinnerets, into a coagulating or precipitating medium, of such character as to immediately coagulate the exterior portion thereof, to such depth as to form what may be termed a skin, with the effect that, as the coagulation and reversion of the viscose within such skin proceeds, such stresses are created that, ultimately. the core comprising the entire substantially cylindrical body of the filament, within such skin, at some stage in its dehydration shrinks in diameter to such an extent as to pull loose from the skin, leaving the latter as a tubular sheath covering such cylindrical core throughout the length of the latter. However, during the desiccation of the structure as a whole, said sheath shrivels so that its exterior surface becomes crinkled and affords numerous irregular fa cets for reflection of light as aforesaid.

My invention includes the various novel features of procedure hereinafter more definitely specified.

I have found that the effect aforesaid is producible by certain relations of the factors of strength of the precipitating bath, the speed of traverse of the filament through bath and time of exposure of the filament to the action of the bath.

Ordinarily, aqueous solutions containing eight percent of sulphuric acid or five percent of hydrochloric acid are considered strong coagulating baths and are commonly used for production of what are termed artificial silk filaments. However, it may be observed in the example of my invention heremafter set forth that the acid stren "h of the bath is more than double such or inary baths.

lVith baths of that character, substantially all of the sulphur primarily chemically combined with the cellulose in viscose is released as free sulphur and is occluded in the mass of cellulose hydrate, forms a dull yellow white surface upon the filament and renders the latter weak and brittle. It is practically impossible to more than partially remove sulphur and its derivatives from such cellulose hydrate by any ordinary process. However, I have discovered that if any suitable coagulating bath is made to include PO ions; filaments of cellulose hydrate formed by coagulating filaments in such baths are practically self-cleansing because the sulphur derivatives are thereby rendered soluble in the bath and automatically eliminated from the filaments. I Such ions may be added to or produced in such baths in any convenient form or manner. However, trisodium phosphate (Na POJ is a cheap vehicle for such ions and may be used in aqueous solution.

Therefore, in one exemplification of my invention, I form a viscose precipitating bath of water containing sixteen and one half percent of H SO,,, in association with one half of one percent of P0 ions, measured as P0,, and cause the filaments of viscose containingtwelve per cent. of cellulose to traverse such bath submerged in a ath thercthrough three and one half feet ong and at the rate of one hundred twenty feet per minute; so that the time of subjection of each portion of the filament to such bath is one and three quarter seconds. However, with a viscose containing fourteen percent, cellulose, with an alkalinity of 3.7 percent. and tri-sodium phosphate content of .42 of the cellulose weight, filaments thereof of 300 denier are precipitated in the manner characteristic of this invention by submersion in a path but one-half inch long in a bath containing 14.7 precent sulphuric acid and one-half percent, tri-sodium phosphate at a temperature of C.

Although the peculiar efl'ect aforesaid may be observed with a filament of three hundred denier, it is markedly characteristic of filaments between six hundred and one thousand denier and I refer to utilize the same in outs of mne hundred denier. It being noted that ordinary viscose contains but seven or ei ht percent of cellulose and is precipitate by an ordinary bath containing from eight to ten percent sul phuric acid; it is obvious that my invention is characterized both by the inclusion of an abnormally lar e percentage of cellulose in the viscose an by inclus on of an abnormally large percentage of acid in the precipitating bath. Although the required acid content of the bath varies inversely with the cellulose content of the viscose, as indicated by the two examples aforesaid, it is characteristic of my invention that the acidity of the precipitation bath shall be at least fifty percent greater than is ordinarily employed.

In said drawin Fig. I is a view of a piece 0 a finished pro invention.

Fi .II is a fragmentary longitudinal sections. view of an extruded viscose filament before coagulation.

Fig. III is a sectional view similar to Fig. II but indicating the coagulation of the exterior of said filament to form the skin aforesaid.

' Fig. IV is a sectional view, similar to Figs. II and III but showing the core of the filament shrunken to such an extent as to be separated from its skin.

Fig. V is a fragmentary sectional view of the structure indlcated in Figs. II to IV inclusive but in the final dessicated state and show the core filament in elevation and the skin sheath thereof in section.

Referring to Fig. I; the com lete roduct of my invention is an artificial t rea which ma be woven, braided, knitted or otherwise embodied in any suitable texture and which includes the substantially smoothly cylindrical solid core filament 1 with the outer continuous imperforate tubular sheath 2 encasin said core in substantiall coaxial spaced relation therewith but having a shriveled crinkled exterior affording multitudinous facets 3 adapted to reflect hght with a scintillating effect.

Figs. II to V inclusive indicate steps in perspective not of my the production of such an artificial textile thread as indicated in Fig. I; by the exemplification of my invention above described.

Fig. II shows the solid homogeneous filament 4 of viscose, which, as extruded through a circular orifice, is substantially cylmdrlcal and of homogeneous structure throughout its mass. Fig. III indicates the firactically instantaneous effect upon the ament of Fig. II incident to its submersion In the bath above contemplated; which effect 18 the coagulation of the exterior of the filament 4 to such depth as to form what may be termed a skin 5. As the coagulation and reversion of the viscose within such skin proceeds,

such stresses are created that, ultimately, the

core com rising the entire substantially cylindrical ody of the filament 4, within such .final stage of its production, both the interior core 1 and exterior-sheath 2 have, of course, shrunken to much smaller diameter than the viscose filament from which they are formed. In fact an extruded viscose filament may shrink to one half its original diameter.

It is most economical to produce such threads in the least possible time of use of the apparatus employed and, therefore, it is desirable to run the extruded filament 4 through the bath at high speed as in the example above set forth. However, the desired effect may be attained in a somewhat weaker bath by longer subjection of the filament thereto; provided that the coagulating action thereof is stron enough to produce the skin eilect describe i.

Moreover, although I prefer to include PO, ions in the bath to avoid the necessity for using other desulphurizing methods and means to cleanse the roduct; of course, threads of the double c aracter above contemplated may be produced in baths which do not contain PO, ions, and such threads be subsequently desulphurized by any of the ordinary methods and means, well known in the art.

Furthermore, although I refer to form such threads from the thiocar onate of cellulose, known as viscose, as above described; containing about twelve per cent of cellulose, in hydrated form; there are at least four other methods of producing artificial colloid filaments in which my invention may be employed to wit, first, in the manufacture of filaments from nitro-cellulose by what is known as the Chardonnet methods and means; second, in what is knownas the cu prammonium process, whereby filaments are formed from a solution of cellulose in an ammoniacal copper oxide; third, in the formation of filaments from a solution of cellulose zinc chloride; and fourth, in the formation of filaments from acetic anhydride. Each of said processes and the methods and means for effecting the same are well known to those skilled in the art and, therefore, my invention may be applied thereto, in

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each case, by using such increased strength of the coagulating or precipitating medium that the ordinary purpose and effect of gradually coagulating the extruded filamentthroughout its mass so as to leave the latter of uniform and unitary composition, which is characteristic of the ordinary processcs, are defeated by the instantaneous production of a substantially,hard and tough skin upon the extruded filament capable of resisting the shrinkage of the gelatinous mass which it incloses; so that the subsequent desiccation of the latter causes it to separate from such skin.

Therefore, I do not desire to limit myself to the precise details of procedure herein set forth, as it is obvious that various modifications may be made therein without departing from the essential features of my invention as defined in the appended claims.

I claim:

1. The process of forming an artificial textile thread including a solid core filament and an outer tubular sheath, encasing said core, which consists in extruding a colloid including hydrated cellulose, through a circular orifice, into a coagulating medium comprising a bath of aqueous liquid containing sixteen and one-half per cent of sulphuric acid, associated with one-half per cent of PO, ions; allowing each portion of said filament to remain submerged in said bath until the exterior thereof is coagulated to form a skin, primarily in unitary relation with the mass of colloid Within it; continuing the reversion and elimination of moisture from said colloid until the core mass within said skin separates from the latter and forms a substantially smoothly cylindrical filament, and said skin forms an outer continuous imperforate tubular sheath, radially separated from said core, but in substantially coaxial, spaced, relation therewith, and having a shriveled crinkled exterior afi'ording multitudinous facets adapted to reflect light with a scintillating effect.

2. The process of forming an artifical textile thread including -a solid core filament and an outer tubular sheath, encasing said core, which consists in extruding a colloid including hydrated cellulose, through a circular orifice, into a coagulating medium comprising a bath of aqueous liquid containing an acid, associated with P0, ions;

said bath being of at least fifty per cent greater acidity than is ordinarily employed to produce a solid filament; allowing each portion of said filament to remain submerged in said bath until the exterior thereof is coagulated to form a skin, primarily in unitary relation with the mass of colloid within it; continuing the reversion and elimination of moisture from said colloid until the core mass within said skin separates from the latter and forms a distinct filament, and said skin forms an outer continuous im rforate tubular sheath, radially separated rom said core, but in substantially coaxial, spaced, relation therewith, and having a shriveled crinkled exterior afl'ording multitudinous and an outer tubular sheath, encasing said core, which consists in extruding a colloid including more than eight per cent of hydrated cellulose, into a coagulating medium comprising a bath of aqueous liquid containing su phuric acid, associated with PO ions; said bath being of at least fifty per cent greater acidity than is ordinarily employed to produce a solid filament; allowing each portion of said filament to remain submerged in said bath until the exterior thereof is coagulated to form a skin, primarily in unitary relation with the mass of colloid within it; continuing the reversion with the mass of moisture from said colloid until the core mass within said skin se arates from the latter and forms a distinct fi ament, and said skin forms an outer continuous tubular sheath, radially separated from said core, but in substantially coaxial relation therewith, and having a shriveled crinkled exterior affording multitudinous facets adapted to reflect light with a scintillating effect.

4. The process of forming an artificial textile thread including a solid core filament and an outer tubular sheath, encasing said core, which consists in extruding a colloid filament including more than eight per cent of hydrated cellulose, into a coagulating medium comprising a bath of aqueous liquid containing sulphuric acid; said bath being of at least fifty per cent greater acidity than is ordinaril employed to produce a solid filament; allbwing each portion of said filament to remain submerged in said bath until the exterior thereof is coagulated to form a skin, primarily in unitary relation with the mass of colloid Within it; continuing the reversion and elimination of moisture from said colloid until the core mass within said skin separates from the latter and forms a distinct filament, and said skin forms an outer continuous tubular sheath, radially separated from said core, but in substantially coaxial relation therewith, and having a shriveled crinkled exterior afi'orcling multitudinous facets adapted to reflect light with a scintillating effect.

5. The process of forming an artifical textile thread including a solid core filament and an outer tubular sheath, encasing said core, which consists in extruding a colloid filament into a coagulating medium; said bath being of at least fifty per cent greater acidity than is ordinarily employed to produce a solid filament; allowing each por- HID lUU

tion of said filament to remain in said medium until the exterior thereof iscoagulated to form a skin, primarily in unitary relation with the mass of colloid within it;'continuing the elimination of moisture from said colloid until the core mass within said skin separates from the latter and forms a distinct filament, and said skin forms an outer continuous tubular sheath, separated from, but encasing, said core, and having a crinkled exterior adapted to reflect light with a scintillating efiect.

6. The process of forming an artificial textile thread including a solid core filament and an outer tubular sheath, encasing said core, which consists in extruding a colloid as an initially unitary filament; coagulating the exterior thereof to form a skin, primariiy in unitary relation with the mass of colloid within it, by suhmerging it in a bath of at least fifty per cent greater acidity than an ordinary viscose precipitating bath; and continuing the coagulation of said colloid until the core mass within said skin Separates from the latter and forms a distinct filament, and said skin forms an outer continuous tubular sheath.

. In testimony whereof, I have hereunto signed my name at Burlington, New Jersey, the twenty-seventh day of January, 1926.

SAMUEL A. NEIDICH.

tion of said filament to remain in said medium until the exterior thereof is coagulated to form a skin, primarily in unitary relation with the mass of colloid within it; con- 5 tinuing the elimination of moisture from as an initially unitary filament; coagulating the exterior thereof to form a skin, primarily in unitary relation with the mass of colloid within it, by submerging it in a bath of at least fifty per cent greater acidity than an ordinary viscose precipitating bath; and continuing the coagulation of said colloid until the core mass within said skin separates from the latter and forms a distinct filament, and said skin forms an outer continuous tubular sheath.

In testimony whereof, I have hereunto signed my name at Burlington, New Jersey, this twenty-seventh day of January, 1926.

SAMUEL A. NEIDICH.

CERTIFICATE OF CORRECTION.

Patent No. 1,643,080.

Granted September 20, 1921, to.

SAMUEL A. NEIDICH.

It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as followa: Page 2, line 79, after "Figs." insert the numeral "1''; page 3, linea 88 and 89, claim 3, strike out the. words "with the mass" and ineert instead the worda "and elimination"; and that the aid Lettera Patent ahould 'be read with these corrections therein that the aame may conform to the record of the came in the Patent 0ft ice.

Signed and aeal-ed thia 11th day of October, A. D. 1927.

Seal.

H. J. Moore, Acting Conaniaaioner of Patenta.

CERTIFICATE OF CORRECTION.

Patent No. 1,643,080.

SAMUEL A. NEIDICH.

It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as follows: Page 2, line 79, after "Figs." insert the numeral "1'' page 3, lines 88 and 89, claim 3; strike out the. words "with the mass" and insert instead the worda "and elimination"; and that the said Letters Patent ahonld be read with these corrections therein that the aame may conform to the record of the caae in the Patent Office.

Signed and sealed thia llth day of October, A. D. 1927.

If. J. Moore, Seal. Acting Commiaaioner of Patents.

Granted September 20, 1921, to. 

